J Mater Sci: Mater Electron (2022) 33:15617–15626

Synthesis, structural, band gap, and optical properties

of Ba3(PO4)2 hierarchical structural materials
Lavuluri Obulapathi1,* , Seelam Harinath Babu1, Boggala Sreenivasulu1, Jaesool Shim2, and
P. C. Nagajyothi2,*

1
Department of Humanities and Sciences, Annamacharya Institute of Technology and Sciences, Rajampet, Andhra Pradesh, India
2
School of Mechanical Engineering, Yeungnam University, Gyeongsan 384541, Republic of Korea

Received: 18 February 2022 ABSTRACT

Accepted: 21 May 2022 Ba3(PO4)2 structure with Rhombohedral phase was prepared by a facile wet
Published online: chemical method. In this experiment, NaOH is used as a surfactant for various
17 June 2022 pH values. The prepared samples were analyzed using several analytical tech-
niques such as XRD, SEM, EDX, UV–Visible absorption, and photoluminescence
Ó The Author(s), under spectroscopy. Orthorhombic (BaHPO4) phase appeared at pH7 and rhombo-
exclusive licence to Springer hedral Ba3(PO4)2 phase formed at pH13 show that the pH value was very
Science+Business Media, LLC, important factor for the final product formation and morphology. The phase
part of Springer Nature 2022 changes have been monitored through the XRD data analysis. EDX analysis
confirms the Ba:P ratios as 3:2. Band gap energy of synthesized microstructure
was found to be 3.60 eV for rhombohedral phase (pH13) and 4.89 eV for
orthorhombic phase (pH7), respectively. Significantly, the prepared sample at
pH13, an intense blue light, emitted a narrow band in the broad band emission
spectra, which have been explained from the transition of 3T1?1A1 in PO43-
ions. In the meantime, an apparent red shift was observed while changing the
excitation wavelengths.

1 Introduction transition metal ions [6, 7], respectively. All of these

Phosphates of metals evolve as a promising photo
material because of their advantages of ecofriendly,
cost-effective, and abundance [1, 2]. Since the 1970’s,
among the several metal phosphates, consideration of
ions Ba3(PO4)2 microcrystals is increasing due to their
optical and electrical characteristics for potential
application in optical, optoelectronic, and mechanical
devices, selective with effective magnetic absorbent
dyes with doping of various lanthanides [3–5] and
selected applications require the nano-sized to have
suitable good phase of host matrices.
To-date, various synthesis approaches such as
coprecipitation, sol–gel, hydrothermal, decomposi-
tion, and electrochemical strategy have been exten-
sively applied to prepare the micro/nano-structured
metal phosphates i.e., Ba3(PO4)2, BaHPO4, and Ba5(-
PO4)3OH, nanocrystal (including nanowire, nano-
rods and hierarchical structures) have attracted
widespread attention [8–10]. In contrast, several

Address correspondence to E-mail: obulapathi.vlsi@gmail.com; pcnnagajyothi@gmail.com

https://doi.org/10.1007/s10854-022-08466-5

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15618
chemical methods are also used to prepare
microstructures with flexible shape and size. The
phase and shape of the material depend on the pH of
the initial solution, experimental temperature, time,
and concentration of the reactant solution.
[2, 6–8, 10, 11].
There are few reports on the synthesis and the
crystal phases of barium phosphate by wet chemical
techniques. But the investigation is not comprehen-
sive and some novel structural analysis and photo-
luminescence characteristics are neglectful, which
needs to be further investigated systematically. As far
we know, most of the literature focus on the mor-
phology evolution of phase transformation of Ba3(-
PO4)2 microcrystal, and there have not been
systematic studies over phase transition and their
structural analysis with photoluminescence.
This study presents rhombohedral phase of Ba3(-
PO4)2 micro structures by a facile wet chemical
method without any additive and investigates the
effect of pH value of the solution on the phase evo-
lution at fixed system reaction temperature. More-
over, the phase changes have been monitored by
XRD, SEM, BET, XPS, UV–Vis diffuse-reflectance,
and photoluminescence spectra.
2 Experimental details
2.1 Materials and synthesis
C4H6BaO4, K2HPO4, and KOH were preliminary
constituents. The final product stoichiometry could
be controlled by changing the pH of initial solution.
Briefly, the starting materials are weighed and mixed
0.003 mol% (0.75 g) of barium acetate and 0.05 g of
CTAB to 50 ml of de-ionized water. Afterward, sep-
arate solution was prepared with 0.0022 mol%
(0.26 g) of ammonium phosphate added in to 50 ml of
DI water. Both the solutions were stirred for 10 min,
and then, 10 mol L-1 NaOH solution was added and
stirred to regulate the alkalinity of the reaction
medium to pH 13. Afterward, the reacted mixture
was kept in water bath at 80 °C for 8 h and wait for
room temperature. End product was dried at 60 °C
under vacuum conditions after centrifuged and
washed sequentially with ethanol and DI water.
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J Mater Sci: Mater Electron (2022) 33:15617–15626
2.2 Characterization
The synthesized samples were characterized by var-
ious analytical tools. XRD patterns were obtained
using a D/max-IIIA, Rigaku, diffractometer with Cu
Ka radiation in the scanning 2h range of 10°–80°.
Morphology and elemental composition analysis
were done by a ZEO 1550 VP FESEM equipped with
an Oxford INCA Energy 300 X-ray EDS system.
Valence states and binding energies of Ba, P, and O
elements were measured using X-ray photoelectron
spectroscopy (XPS; ESCALAB250), through binding
energies optimized based on specimen charging by
referring to the C(1s) peak position at 284.40 eV. The
BET surface area was measured by nitrogen absorp-
tion using a Micromeritics ASAP 2020 analyzer. The
excitation and emission spectra were measured using
an FLS-920 time-resolved and steady-state fluores-
cence spectrometer (Edinburgh Instruments) equip-
ped with a 450 W Xe lamp, a TM300 excitation
monochromator, a double TM300 emission
monochromator, and a Red PMT.
3 Results and discussion
3.1 Phase identification and structural
analysis
XRD profiles of the synthesized samples at various
pH values are shown in Fig. 1. It can be seen that the
phase of the prepared samples was significantly
affected by pH value of initial solution and prepared
samples were well crystallized. The diffractions
peaks of the samples prepared with pH of 6, 7, and 8
were well matched with the reported BaHPO4
structures of orthorhombic phase (JCPDS card No.
01-72-1370), and pH value of 10, 11, 12, and 13 sam-
ples structure was well matched with rhombohedral
structure of Ba3(PO4)2 (JCPDS card No. 25-028). These
results are shown in Fig. 2. The phase transformation
was explained based on the values of pH in the
NH4H2PO4 ionized method [12]. The processes of
ionization reaction can be explained with the help of
below three chemical equations [12]:
J Mater Sci: Mater Electron (2022) 33:15617–15626 15619

þ
HPO2 3
4  H þ PO4 ð3Þ

The above reaction scheme contains several H?

ions when the pH value was 6 or below 6 resulting in
the development of H2PO4-, and HPO42- ions.
Transformations of equations from 1 to 3 have been
difficult to happening and easily forming a low
concentration of PO43-. Based on the phase formation
law, less concentration of PO43- is advantageous for
the development of orthorhombic phase in BaHPO4
[12]. For high pH ([ 6) value, a few H? ions will
support positively for reaction equilibrium, causing
more concentration of PO43- [8, 12]. An increase of
the concentration of PO43- induced by the initial pH
value favors the formation of rhombohedral phase
Ba3(PO4)2. The formation of the crystal will be
examined by SEM analysis [8, 12].

3.2 Surface morphology analysis

Fig. 1 XRD patterns of samples prepared at different pH values
Figure 3 shows the microstructures of the obtained
samples at various pH values and shows that at
pH = 6, well-dispersed semi-hexagonal irregularly
shape (uneven sizes)-like quadrilateral boxes micro-
crystals with well-defined edges sand sharp corners.
When the pH value was 7, the material could
appropriately self-establish into well-organized 1-D
Orthorhombic structure. The anisotropic growth of
orthorhombic morphology of BaHPO4 (Fig. 2) is
attributed to the high chemical potential of PO43- in
the pH of 7. At pH = 8, the morphology of BaHPO4
splitting into double orthorhombic undersized but
still remained as 1-D orthorhombic structures, while
the diameter splitting to 400–800 nm and the length
decreased to 10–30 mm (Fig. 3). It seems that pH
condition 7 is suitable for the growth of one dimen-
sion quadrilateral box (orthorhombic morphology)
Fig. 2 XRD patterns and corresponding JCDPS card numbers of with smooth surface.
orthorhombic-pH7 and Rhombohedral-pH 13 samples When pH value increased to 9, morphology of the
Ba3(PO4)2 formed as nanorods and aggregated
instinctively to form clusters with micro sizes due to

NH4 H2 PO4  NHþ
4 þ H2 PO4 ð1Þ high surface energy [13]. It indicates that
microstructures are responsible for developing
H2 PO þ 2
4  H þ HPO4 ð2Þ
flower-like structures. Consequently, conditions
became quite different when the pH value continu-
ously increased (pH = 10, 11 ,and 12). When pH = 10,

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15620 J Mater Sci: Mater Electron (2022) 33:15617–15626

Fig. 3 SEM images of

samples prepared at various
pH values

11, the uniform microrods of Ba3(PO4)2 completely flower-/plate-like structures with few nano meter
disappeared and numerous irregular plate-like large size are shown in Fig. 3. At pH = 13, the formation of
particles of Ba3(PO4)2 have been observed which is sharp microstructured flower-like 3D Ba3(PO4)2 was
shown in Fig. 3. After pH = 12, clear partial observed, these plate-like particles were

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J Mater Sci: Mater Electron (2022) 33:15617–15626
Fig. 4 EDAX pattern of Rhombohadrel-pH13
amalgamated collectively to form flower-/plate-like
structures due to Ostwald ripening [14]. XRD profiles
also confirmed that the orientation growth control of
inorganic crystals would terminate at higher pH
values. Both XRD and SEM results were well coin-
cided at various pH values.
3.3 EDX and XPS analysis
Figure 4 shows the EDAX analysis of prepared
samples (pH 13) and it confirms the presence of all
elements such as O, P, and Ba. Figure 5 shows the
XPS analysis of the samples prepared at pH = 13 for
further confirmation of the composition. XPS spec-
trum confirms the Ba, O, and P elements without any
impurities and which is well matched with the EDAX
analysis. C(1s) peak of 284.6 eV is used to regulate
the binding energies of the other elements as shown
in Fig. 5b–d, where the values shown for O (1s,
538.21 eV), P (2p, 133.71 eV), and Ba (3d, 780.30 and
759.69 eV) match with the literature [15].
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15621
3.4 Brunauer–Emmett–Teller (BET)
analysis
Figure 6 shows the BET analysis of orthorhombic (pH
7) and rhombohedral (pH 13) phases samples. The
surface area of rhombohedral (Rh-pH 13) phases
barium phosphate (Ba3O9P2) was found to be 12.24
m2g-1 and the pore volume was 0.0089195 cm3g-1.
The specific area for Orthorhombic (Orth-pH 7)
barium phosphate (BaHPO4) was 5.2278 m2/g. As
shown in Fig. 6, the two compounds present a very
similar behavior but the Orthorhombic (pH 7)
absorbs more rapidly than the rhombohedral (pH13).
The pore-size dispersals calculated by the Barrett–
Joyner–Halenda method (Fig. 6c, d) for both phase
materials confirm the presence of well-developed
mesoporosity with very narrow pore-size scattering
centered at 43.925 and 40.111 nm for Orthorhombic
(pH 7) and rhombohedral (pH13) phases of synthesis
materials, respectively. As expected, the high pH
value of sample has reduced the surface area and
porosity of both materials, significantly.
3.5 Optical band gap
The linear absorption coefficient, a, is related to
photon energy ht through the well-known Tauc’s
relationship [16].

n=2
ahv ¼ A1 hv  Eg ; ð4Þ
where m is the frequency of photon energy and A1 is a
band edge constant.

n
½ahv2 ¼ A1 hv  Eg ð5Þ
The optical band gap was calculated by the
exploration of linear portion of aht vs. ht as shown in
Fig. 7. The x-axis intercept of linear curve to be found
as band gap is around 3.60 eV for rhombohedral
15622 J Mater Sci: Mater Electron (2022) 33:15617–15626

Fig. 5 a XPS full spectrum of Ba3(PO4)2 sample, b XPS P2p spectrum, c XPS Ba3d spectrum, and d XPS for O1s

phase (pH13) and 4.89 eV for orthorhombic phase
(pH7). Here, different crystal phases lead to different
light absorption activities of rhombohedral and
orthorhombic phase of Ba3(PO4)2 structure which can
be carried out with appropriate photo energy
(\ 400 nm).
3.6 Photoluminescence analysis
Figures 8 and 9 exhibit both the excitation and
emission spectra of rhombohedral (Rh-pH13) phases
of Ba3(PO4)2. In the spectra of emission in Fig. 9a and
its enlarge spectra Fig. 9b, shown with the intense

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J Mater Sci: Mater Electron (2022) 33:15617–15626 15623

Fig. 6 a–d Nitrogen adsorption–desorption isotherms orthorhombic-pH7 and Rhombohedral-13, respectively

centered peak at 313 nm emission, with red shift of
2–4 nm is observed. Entire phenomena may be
endorsed that the size of the particles is in
the nanometer scale. The small size effect, Surface
and boundary effect, quantum size effect, dielectric
confinement effect, and macroscopic quantum tunnel
effect are the five main specific effects of nano
materials. From these five, first two are well investi-
gated for their effects on luminescence properties
[17]. Normally, the happening of red shifts most
likely be endorsed to the surface and interface effect
which could increase the crystal field resulting in the
energy levels or reducing the band gap. The small
size effect can generate two results. One is the crystal

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15624
Fig. 7 The Tauc’s plots for a orthorhombic phase (pH7) and
b Rhombohedral phase (pH13) Ba3(PO4)2 samples
periodic boundary conditions which will be
destroyed due to reduction of particle size, observing
the enlargement of emission peaks. Second one is the
related specific surface area which will amplify
promptly and puts many surface atoms in an
exposed state, so that main surface defects are
unavoidable. Consequently, the spectral composition
may change.
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J Mater Sci: Mater Electron (2022) 33:15617–15626
Oemi = (nm)
400
Relative Intensity (a.u)
405
410
415
420
440
444
447
260 280 300 320 340 360 380 400
Wavelength (nm)
Fig. 8 Excitation spectra of Rhombohedral phase (pH13)
Ba3(PO4)2 nanocrystal
4 Conclusions
In summary, we report a facile ligand-free strategy
for the synthesis of dual phases of Ba3(PO4)2
nanocrystal. Interestingly, the orthorhombic (Orth-
pH7) and rhombohedral (Rh-pH13) phases can be
selectively obtained by adjusting the synthesis
parameters. Furthermore, the underlying mechanism
of phase transformation of orthorhombic (orth-pH7)
to rhombohedral (Rh-pH13) phases was elucidated.
The energy gap is found to be 4.89 eV (Ortho-pH7)
and 3.60 eV (Rh-13) samples, respectively. Interest-
ingly, the as-synthesized dual phase order of Ba3(-
PO4)2 was found red shift in their narrow blue
emission bands within a broad band from 360 to
480 nm, by monitoring different excitation wave-
lengths for the first time, for which complex ions
luminescence from different electronic structures and
their transition probabilities from the excited state to
the ground state. This work provides a more
promising strategy with superiorities of low cost in
synthesis, environment friendly, and adaptive for
large-scale fabrication with controllable particle size,
morphology, and stability.
J Mater Sci: Mater Electron (2022) 33:15617–15626
Fig. 9 a Emission spectra and b enlarge emission spectra of
Rhombohedral phase (pH13) nanocrystal
Acknowledgements
P.C. Nagajyothi and Jaesool Shim acknowledges the
National Research Foundation of Korea (NRF) Grants
funded by the Korean government
(2020R1A4A1019227 and 2020R1A2C1012439).
Author contributions
LO, SHB have contributed equally to this work. LO
and SHB guided all the experimental design, and led
the manuscript preparation. JS and PCN did the data
analysis, and prepared the draft manuscript. All
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15625
authors have given approval to the final version of
the manuscript.
Data availability
Data will be made available on reasonable request of
the authors.
Declarations
Conflict of interest All the authors do not have any
possible conflicts of interest.
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